CN113817136A - 一种高固含量水性聚氨酯及其制备方法 - Google Patents
一种高固含量水性聚氨酯及其制备方法 Download PDFInfo
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- CN113817136A CN113817136A CN202010585065.2A CN202010585065A CN113817136A CN 113817136 A CN113817136 A CN 113817136A CN 202010585065 A CN202010585065 A CN 202010585065A CN 113817136 A CN113817136 A CN 113817136A
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- aqueous polyurethane
- polyurethane
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Classifications
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- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
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- C—CHEMISTRY; METALLURGY
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明涉及聚氨酯材料领域，特别是一种高固含量水性聚氨酯及其制备方法。按重量份计，异氰酸酯类40～60份，多元醇类60～80份，催化剂类0.2～0.5份，醇类扩链剂类3～10份，胺类扩链剂类5～8份，亲水性扩链剂类5～10份，小分子扩链剂类1～10份，封端剂类1～3份，成盐剂类3～5份，溶剂类30～50份，乳化剂100～200份。本发明基于多元异氰酸酯类的异氰酸根可以与羟基、胺基、水等活性基团发生Michael加成反应的特点，采用多种扩链剂对聚氨酯预聚体进行扩链加成反应，最后通过中和乳化制备出具有高固含量的水性聚氨酯。此外，由于该聚氨酯为水性，具有绿色环保的性能。
Description
技术领域
本发明涉及聚氨酯材料领域，特别是一种高固含量水性聚氨酯及其制备方法。
背景技术
聚氨酯作为一种新型的高分子聚合材料，既能弥补传统的丙烯酸树脂耐候性差的短板，又能弥补水性环氧树脂容易开裂的缺点，正在被越来越广泛的应用在建筑、汽车、船舶、高铁、木材、皮革等涂料领域。油性聚氨酯由于挥发性有机物含量高，对环境污染严重，不符合“绿水青山”的发展理念，正在被逐渐淘汰。水性聚氨酯虽然满足环保的要求，但其固含量低的不足严重制约着它的使用。
CN109824850A公开了一种双组分水性聚氨酯及其制备方法和应用，其双组分使用工序繁琐，且还有添加成膜助剂、流平剂、消泡剂等价格高昂的助剂； CN110229302A公开了一种侧链含硅原子的水性聚氨酯乳液及其制备方法，其固含量处于30％～40％之间，CN110128615A公开了一种水性聚氨酯及其制备方法和应用，其固含量虽然高于其他公开资料，达到40％，但还是处于相对较低的水平； CN110372840A公开了一种无机-有机复合改性交联型水性聚氨酯乳液及其制备方法，其通过添加无机材料SiO2来增加固含量，这个方法并没有从本质上解决水性聚氨酯固含量低这一问题。
多元异氰酸酯中的异氰酸根可以羟基、胺基、硅烷基等发生Michael加成，该反应可以迅速增长碳链，是聚合物的分子量得到极大的增加，传统的水性聚氨酯仅仅利用了异氰酸根与多元醇中的羟基加成，或者加以亲水加成来扩张碳链，但这毕竟是有限的。本发明通过引入小分子扩链剂，该扩链剂含有的多个羟基可以和羧基以及异氰酸根再次加成，这样就可以对聚氨酯预聚体进行再次扩链，使得分子量进一步增加，最终提高水性聚氨酯的固含量。
发明内容
本发明的目的在于克服油性聚氨酯环境污染的问题，提供了一种水性聚氨酯。
本发明的另一目的在于克服现有水性聚氨酯固含量低的问题，提供了一种高固含量的水性聚氨酯的制备方法。
本发明的另一目的在于一种高固含量水性聚氨酯应能满足耐候性、不易开裂、耐酸碱性等要求。
本发明的目的通过以下技术方案予以实现：
一种高固含量水性聚氨酯及其制备方法。按重量份计，异氰酸酯类40～60份，多元醇类60～80份，催化剂类0.2～0.5份，醇类扩链剂类3～10份，胺类扩链剂类5～8 份，亲水性扩链剂类5～10份，小分子扩链剂类1～10份，封端剂类1～3份，成盐剂类3～5份，溶剂类30～50份，乳化剂100～200份。
优选地，异氰酸酯类为多元类，再优选地，异氰酸酯为二元类异氰酸酯，包括对苯二异氰酸酯、萘二异氰酸酯、异佛尔酮二异氰酸酯、间苯二亚甲基二异氰酸酯、1，4-环己基二异氰酸酯、三甲基己二异氰酸酯、甲苯-2，5-二异氰酸酯、 1，4-环己烷二甲基二异氰酸酯，更优选地，异氰酸酯为对苯二异氰酸酯、萘二异氰酸酯、异佛尔酮二异氰酸酯、1，4-环己基二异氰酸酯。
优选地，多元醇类为聚酯型多元醇和聚醚型多元醇，更优选地，聚酯型多元醇包括聚癸二酸乙二醇酯二醇、聚己二酸丙二醇酯二醇、聚邻苯二甲酸-1，6-己二醇聚酯二醇；聚醚型多元醇包括聚丁二醇、聚氧化丙烯二醇、聚氧化丙烯三醇。
优选地，催化剂为锡类催化剂，更优选地，锡类催化剂包括二乙酸二丁基锡、二(十二烷硫基)二丁基锡、二(异辛基马来酸)二丁基锡。
优选地，醇类扩链剂为二元、三元类，更优选地，醇类扩链剂为二元醇类，包括1，3-丙三醇、1，5-戊二醇、1，7-庚二醇。
优选地，胺类扩链剂为脂肪族二元胺，包括1，2-丙二胺、1，4-戊二胺。
优选地，亲水性扩链剂为磺酸型或羧酸型物质，更为优选地，亲水性扩链剂为羧酸型物质，包括2，2-二羟甲基丙酸、2，2-二羟甲基丁酸、2，5-二羟基苯甲酸。
优选地，小分子扩链剂为双季戊四醇、三季戊四醇。
优选地，封端剂为硅烷类化合物，包括正辛基三乙氧基硅烷、N-癸基三乙氧基硅烷、十六烷基三乙氧基硅烷、正十八烷基三乙氧基硅烷，更优选地，硅烷封端剂为十六烷基三乙氧基硅烷、正十八烷基三乙氧基硅烷。
优选地，成盐剂为具有碱性的胺类物质，再优选地，成盐剂包括三丙胺、三戊胺、三庚胺、三辛胺，更优选地，成盐剂为三丙胺、三戊胺。
优选地，溶剂为有机溶剂，包括丙酮、丁酮、甲苯，更优选地，溶剂为丙酮。
优选地，乳化剂为去离子水。
上述一种高固含量水性聚氨酯的制备方法，包括以下步骤：a.将多元醇类，醇类扩链剂类，胺类扩链剂类，亲水性扩链剂类，小分子扩链剂类使用前在 100～120℃在真空干燥2～3h；b.将溶剂、异氰酸酯类和多元醇类按比例加放入有搅拌器、温度计、回流冷凝管的干燥三口瓶中；c.继续加入化一定量的锡类催化剂，在N2保护下，40～60℃反应20～40min，升温至70～80℃继续反应60～80min；d. 按比例加入亲水性扩链剂、醇类扩链剂升温至90～95℃反应40～50min，继续按比例加入胺类扩链剂反应30～40min；e.按比例加入小分子扩链剂继续反应30～40min 后加入一定量成盐剂，反应5～10min后加入一定量封端剂；f.按比例加入乳化剂搅拌20～30min后，蒸出溶剂，冷却过滤，得到水性聚氨酯乳液。
与现有技术相比，本发明具有以下技术效果：
现有油性聚氨酯存在VOC含量高，污染环境等问题，水性聚氨酯又存在固含量低以及耐候性、耐酸碱性差的问题。本发明提供的高固含水性聚氨酯，一方面可以解决环境污染的问题，是一种绿色环保的新型材料，另一方面可以提供较高的固含量，可以满足多方面的用途，如建筑、汽车、船舶、高铁、木材、皮革等涂料领域，具有优异的耐紫外老化、耐酸碱等性能。
具体实施方式
为使本发明的目的、发明内容和优点更加清楚，下面将结合具体实施例对本发明的技术方案进行详细的描述。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所得到的所有其它实施方式，都属于本发明所保护的范围。
除特殊说明，本发明中所用的设备均为常规实验设备，所用的试剂均为市售可得。
实施例1～5选用的配料见下表1
表1 各实施例的原料配比
实施例1实施例1～5按照如下步骤制备：
a.将多元醇类，醇类扩链剂类，胺类扩链剂类，亲水性扩链剂类，小分子扩链剂类使用前在100～120℃在真空干燥2～3h；
b.将溶剂、异氰酸酯类和多元醇类按比例加放入有搅拌器、温度计、回流冷凝管的干燥三口瓶中；
c.继续加入化一定量的锡类催化剂，在N2保护下，40～60℃反应20～40min，升温至70～80℃继续反应60～80min；
d.按比例加入亲水性扩链剂、醇类扩链剂升温至90～95℃反应40～50min，继续按比例加入胺类扩链剂反应30～40min；
e.按比例加入小分子扩链剂继续反应30～40min后加入一定量成盐剂，反应 5～10min后加入一定量封端剂；f.按比例加入乳化剂搅拌20～30min后，蒸出溶剂，冷却过滤，得到水性聚氨酯乳液。
根据《GB/T 1725-2007色漆、清漆和塑料不挥发物含量的测定》、《GB/T 1865-2009色漆和清漆人工气候老化和人工辐射曝露滤过的氙气辐射》、《GB 1763-79(89)漆膜耐化学试剂测定法》的相关要求，对实施例1～5所制得的水性聚氨酯进行固含量、耐候性及耐酸碱性的测试，测试结果见表2。
表2 实施例1～5测试结果
实施例1～5所制得的水性聚氨酯都具有优异的耐候、耐酸碱等性能，且它们都具有较高的固含量，最高可达实施例2的47.1％，实施例2之所以有如此高的固含量，主要是因为它所用的异氰酸酯为萘二异氰酸酯，作为芳香族异氰酸酯，它有着比脂肪族异氰酸酯更高的反应活性，更容易与多元醇及各类扩链剂进行加成反应，并且萘二异氰酸酯具有中心对称分子的特征，这意味着它的两个异氰酸根具有相等的反应几率，使得它能够更平稳地进行扩链反应，最终得到较高固含量的水性聚氨酯。
上述实施例为本发明较佳的几个实施方式，但本发明的实施方式并不受上述实施例的限制，本领域的普通技术人员可以理解：在不脱离本发明的原理和宗旨的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由权利要求及其等同物限定。
Claims (10)
1.一种高固含量水性聚氨酯及其制备方法，其特征在于，按重量份计，所述高固含水性聚氨酯需组分包括：异氰酸酯类40～60份，多元醇类20～30份，催化剂类0.2～0.5份，醇类扩链剂类3～10份，胺类扩链剂类5～8份，亲水性扩链剂类5～10份，小分子扩链剂类40～50份，封端剂类1～3份，成盐剂类3～5份，溶剂类30～50份。
2.根据权利要求1所述高固含水性聚氨酯，其特征在于，异氰酸酯为多元类，包括二元异氰酸酯、三元异氰酸酯等，所述异氰酸酯为对苯二异氰酸酯、萘二异氰酸酯、异佛尔酮二异氰酸酯、间苯二亚甲基二异氰酸酯、1，4-环己基二异氰酸酯、三甲基己二异氰酸酯、甲苯-2，5-二异氰酸酯、1，4-环己烷二甲基二异氰酸酯、三苯基甲烷三异氰酸酯、L-赖氨酸三异氰酸酯中的一种或多种。
3.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，多元醇类为聚酯型多元醇和聚醚型多元醇，聚酯型多元醇可以提供良好的耐候性、耐磨性、耐化学性及韧性，聚醚型多元醇可以提供优良的柔顺性、耐水解性，所述聚酯型多元醇为聚癸二酸乙二醇酯二醇、聚癸二酸丙二醇酯二醇、聚癸二酸丁二醇酯二醇、聚己二酸丙二醇酯二醇、聚邻苯二甲酸-1，6-己二醇聚酯二醇中的一种或几种；聚醚型多元醇为聚丁二醇、聚氧化丙烯二醇、聚氧化丙烯三醇中的一种或几种。
4.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，催化剂为锡类催化剂，胺类与锡类催化剂以不同比例混合使用时，具有协同效应，催化效率大大增加，所述锡类催化剂为二乙酸二丁基锡、二(十二烷硫基)二丁基锡、二(异辛基马来酸)二丁基锡中的一种或几种。
5.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，扩链剂包括醇类扩链剂和胺类扩链剂，醇类扩链剂主要为二元、三元醇类，对调节聚氨酯分子量及软硬链段的比例，形成高分子量的线型体或线型大分子，提高力学性能及耐介质性有重要的作用，所述醇类扩链剂为1，3-丙三醇、1，5-戊二醇、1，7-庚二醇、丙三醇、1，2，4-丁三醇中的一种或几种。胺类扩链剂为脂肪族二元胺，能够很明显的增大聚氨酯的分子量，胺类扩链剂的扩链反应非常迅速，所述胺类扩链剂为1，2-丙二胺、1，4-戊二胺中的一种或几种。
6.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，亲水性扩链剂为磺酸型或羧酸型物质，能在聚氨酯大分子主链上引入亲水性基团的扩链剂，是水性聚氨酯合成中使用的功能性单体，所述磺酸型亲水扩链剂为2，5-二羟基苯磺酸、甲氨基磺酸、乙基氨基磺酸中的一种或几种；羧酸型亲水扩链剂为2，2-二羟甲基丙酸、2，2-二羟甲基丁酸、2，5-二羟基苯甲酸中的一种或几种。
7.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，小分子扩链剂主要为小分子醇类，它主要与多余的羧基、胺基、异氰酸根等加成反应，起到增加固含量的作用，所述小分子扩链剂为双季戊四醇、三季戊四醇中的一种或几种。
8.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，封端剂为硅烷类化合物，主要起消除端基官能团活性的作用，所述硅烷类封端剂为正辛基三乙氧基硅烷、N-癸基三乙氧基硅烷、十六烷基三乙氧基硅烷、正十八烷基三乙氧基硅烷中的一种或几种。
9.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，成盐剂为具有碱性的胺类物质，由于引入羧基后，羧基电离度小，必须与碱性物质中和成盐后才具有较强的亲水性，所述胺类成盐剂为三丙胺、三戊胺、三庚胺、三辛胺中的一种或几种。
10.根据权利要求1所述高固含水性聚氨酯及其制备方法，其特征在于，制备方法包括以下步骤：a.将多元醇类，醇类扩链剂类，胺类扩链剂类，亲水性扩链剂类，小分子扩链剂类使用前在100～120℃在真空干燥2～3h；b.将溶剂、异氰酸酯类和多元醇类按比例加放入有搅拌器、温度计、回流冷凝管的干燥三口瓶中；c.继续加入化一定量的锡类催化剂，在N2保护下，40～60℃反应20～40min，升温至70～80℃继续反应60～80min；d.按比例加入亲水性扩链剂、醇类扩链剂升温至90～95℃反应40～50min，继续按比例加入胺类扩链剂反应30～40min；e.按比例加入小分子扩链剂继续反应30～40min后加入一定量成盐剂，反应5～10min后加入一定量封端剂；f.按比例加入乳化剂搅拌20～30min后，蒸出溶剂，冷却过滤，得到水性聚氨酯乳液。
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